CN109320254A - A kind of SiC reinforcement aluminium nitride ceramics and preparation method thereof - Google Patents
A kind of SiC reinforcement aluminium nitride ceramics and preparation method thereof Download PDFInfo
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The invention discloses a kind of SiC reinforcement aluminium nitride ceramics, the weight percent of the ceramics is formed are as follows: aluminium nitride 85%~93%, silicon carbide 5%~10% and silicon 2%~5%.Also disclose preparation method, comprising: (1) silicon carbide and silicon are added in deionized water, then add binder, 45~90min of ball milling mixing obtains silicon carbide-silicon slurry；(2) silicon carbide-silicon slurry is spray-dried using atomizing granulating technology, obtains silicon carbide-silicon amyloplastid；(3) into silicon carbide-silicon amyloplastid be added aluminium nitride amyloplastid, be sieved, be uniformly mixed, suppressed under the conditions of 60~100MPa, then under the conditions of 80~90 DEG C drying 12~for 24 hours, obtain aluminium nitride biscuit；(4) it will be put into sintering furnace after above-mentioned aluminium nitride biscuit, be sintered under the conditions of 1600~2300 DEG C, and keep the temperature 2~5 hours under the conditions of 100~1000 DEG C, obtain SiC reinforcement aluminium nitride ceramics.There is higher hardness, fracture toughness and bending strength using ceramics made of the method for the present invention.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of SiC reinforcement aluminium nitride ceramics and its preparation side
Method.
Background technique
Ceramics needed for mechanical seal industry, it is desirable that material have high intensity, high tenacity, low creep properties, abrasion-resistant wear,
Corrosion resistance and good inoxidizability.Silicon carbide ceramics has excellent mechanical performance, lower thermal expansion coefficient and height
The coefficient of heat conduction so that silicon carbide ceramics shows excellent thermal shock resistance, but also there is high thermal stability, good
Corrosion-resistant, scratch-resistant performance, therefore mechanical seal ring field can be widely applied to.
Due to silicon carbide chemical bond characteristics, ceramic post sintering condition is more harsh.Normal pressure-sintered appearance is so that silicon carbide
Ceramic industry metaplasia produces to have obtained extensive realization.Normal pressure-sintered includes solid-phase sintering and liquid-phase sintering, and solid-phase sintering needs higher
Sintering temperature (2100 DEG C of >) so that silicon carbide whisker particle size is larger, Ceramic Fracture mode is also mostly transgranular fracture, causes to break
It is lower to split toughness.Generally there are commonly B-C, Al-B-C, Al for sintering aid2O3、Al2O3-Re2O3Deng, wherein Re represent rare earth member
The one or more of element；But these sintering aids are waited at high temperature and silicon carbide reacts or volatile ratio is more serious, so that
Sintered Quality loss is serious, is unfavorable for densified sintering product.In recent years it has been found that since silicon carbide and aluminium nitride material are in atom
It is similar on size, molecular weight, density and crystal structure, it will form solid solution within the temperature range of 1800~2100 DEG C；With
The formation of solid solution, sintering activity, microstructure, mechanical property and the inoxidizability of material largely improved
And raising.But because aluminium nitride and water can react in the case where mechanical stirring, aluminium nitride is used to help for sintering at present
The technique that agent prepares silicon carbide ceramics mostly uses ethyl alcohol for solvent progress ball mill mixing, but the ceramics that this technique is produced
Higher cost, when mist projection granulating, are easy to happen explosion.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of SiC reinforcement aluminium nitride ceramics and preparation method thereof, energy
Enough solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of SiC reinforcement aluminium nitride ceramics and preparation method thereof, to overcome existing skill
Deficiency in art.
To achieve the above object, the invention provides the following technical scheme:
A kind of SiC reinforcement aluminium nitride ceramics, the weight percent composition of the ceramics are as follows: aluminium nitride 85%~93%,
Silicon carbide 5%~10% and silicon 2%~5%.
The present invention also provides a kind of preparation methods of SiC reinforcement aluminium nitride ceramics, comprising the following steps:
(1) silicon carbide and silicon are added in deionized water, then add binder, 45~90min of ball milling mixing is carbonized
Silicon-silicon slurry；
(2) silicon carbide-silicon slurry is spray-dried using atomizing granulating technology, obtains silicon carbide-silicon and makes powder
Grain, wherein drying temperature is 80~100 DEG C；
(3) aluminium nitride amyloplastid is added into above-mentioned silicon carbide-silicon amyloplastid, is sieved, is uniformly mixed, in 60~100MPa
Under the conditions of suppressed, then under the conditions of 80~90 DEG C drying 12~for 24 hours, obtain aluminium nitride biscuit；
(4) it will be put into sintering furnace after above-mentioned aluminium nitride biscuit, be sintered under the conditions of 1600~2300 DEG C, and
2~5 hours are kept the temperature under the conditions of 100~1000 DEG C, obtains SiC reinforcement aluminium nitride ceramics.
Preferably, in step (3), the preparation method of the aluminium nitride amyloplastid includes: that carbon black 1) is dispersed in one
In quantitative water, then disperse aluminum nitrate and additive dissolution in carbon black solution in proportion, after mixing, 100~
It is heated at a temperature of 600 DEG C, solution obtains predecessor after reacting；2) the flowing nitrogen by the predecessor at 1200~1600 DEG C
60~600min of carbon thermal reduction in gas or ammonia atmosphere obtains carbothermic reduction reaction product；3) carbothermic reduction reaction is produced
Object, which is passed through, removes 30~600min of carbon in 500~800 DEG C of at a temperature of oxidation, obtains aluminium nitride amyloplastid.
Preferably, the binder is selected from one of polyvinyl alcohol, polyvinyl butyral, methylcellulose.
Preferably, the weight of the binder is the 0.1~0.2% of silicon carbide and silicon gross weight.
Preferably, in step 1), the additive is urea, ammonium nitrate, nitric acid.
Compared with the prior art, the advantages of the present invention are as follows: in the present invention, by the way that silicon carbide and silicon is added, greatly improve
Hardness, fracture toughness and the bending strength of aluminium nitride ceramics in the present invention.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of SiC reinforcement aluminium nitride ceramics, the weight percent composition of the ceramics are as follows: aluminium nitride
85%~93%, silicon carbide 5%~10% and silicon 2%~5%, it is preferred that aluminium nitride 91.5%, silicon carbide 6% and silicon
2.5%.
The invention discloses the preparation methods of above-mentioned SiC reinforcement aluminium nitride ceramics, comprising the following steps:
(1) silicon carbide and silicon are added in deionized water, then add binder, 45~90min of ball milling mixing is carbonized
Silicon-silicon slurry；
(2) silicon carbide-silicon slurry is spray-dried using atomizing granulating technology, obtains silicon carbide-silicon and makes powder
Grain, wherein drying temperature is 80~100 DEG C；
(3) aluminium nitride amyloplastid is added into above-mentioned silicon carbide-silicon amyloplastid, is sieved, is uniformly mixed, in 60~100MPa
Under the conditions of suppressed, then under the conditions of 80~90 DEG C drying 12~for 24 hours, obtain aluminium nitride biscuit；
(4) it will be put into sintering furnace after above-mentioned aluminium nitride biscuit, be sintered under the conditions of 1600~2300 DEG C, and
2~5 hours are kept the temperature under the conditions of 100~1000 DEG C, obtains SiC reinforcement aluminium nitride ceramics.
In above-mentioned steps (1), the binder in polyvinyl alcohol, polyvinyl butyral, methylcellulose one
Kind, and the weight of the binder is the 0.1~0.2% of silicon carbide and silicon gross weight.
In above-mentioned steps (3), the preparation method of the aluminium nitride amyloplastid include: 1) carbon black is dispersed in it is a certain amount of
Water in, then by aluminum nitrate and additive dissolution be scattered in carbon black solution in proportion, after mixing, at 100~600 DEG C
At a temperature of heat, solution obtains predecessor after reacting；2) by the predecessor 1200~1600 DEG C flowing nitrogen or
60~600min of carbon thermal reduction in ammonia atmosphere obtains carbothermic reduction reaction product；3) the carbothermic reduction reaction product is passed through
30~600min of carbon is removed in 500~800 DEG C of at a temperature of oxidation, obtains aluminium nitride amyloplastid.
Wherein, in step 1), the additive is urea, ammonium nitrate, nitric acid.
Embodiment
The preparation method of SiC reinforcement aluminium nitride ceramics, comprising the following steps:
(1) silicon carbide and silicon are mixed according to 6% and 2.5% ratio, is added in 100 parts of deionized waters, then add
0.15% polyvinyl alcohol, ball milling mixing 60min obtain silicon carbide-silicon slurry；
(2) silicon carbide-silicon slurry is spray-dried using atomizing granulating technology, obtains silicon carbide-silicon and makes powder
Grain, wherein drying temperature is 80 DEG C；
(3) the aluminium nitride amyloplastid that the above method is prepared is added into silicon carbide-silicon amyloplastid, sieving, mixing is
It is even, it is suppressed under the conditions of 80MPa, is then dried under the conditions of 80 DEG C for 24 hours, obtain aluminium nitride biscuit；
(4) it will be put into sintering furnace, be sintered under the conditions of 1850 DEG C, and in 400 DEG C of items after above-mentioned aluminium nitride biscuit
5 hours are kept the temperature under part, obtains SiC reinforcement aluminium nitride ceramics.
In the present invention, uses the Vickers hardness of HV-5 type Vickers test aluminium nitride ceramics for 16.2GPa, use
Instrong3382 universal electrical experimental machine test aluminium nitride ceramics bending strength and fracture toughness be respectively 480MPa and
5.12MPa·m1/2, by the way that silicon carbide and silicon is added, substantially increase in the present invention hardness, fracture toughness of aluminium nitride ceramics and
Bending strength.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (6)
1. a kind of SiC reinforcement aluminium nitride ceramics, which is characterized in that the weight percent of the ceramics forms are as follows: aluminium nitride
85%~93%, silicon carbide 5%~10% and silicon 2%~5%.
2. the preparation method of SiC reinforcement aluminium nitride ceramics according to claim 1, which is characterized in that including following step
It is rapid:
(1) silicon carbide and silicon are added in deionized water, then add binder, 45~90min of ball milling mixing obtains silicon carbide-
Silicon slurry；
(2) silicon carbide-silicon slurry is spray-dried using atomizing granulating technology, obtains silicon carbide-silicon amyloplastid,
In, drying temperature is 80~100 DEG C；
(3) aluminium nitride amyloplastid is added into above-mentioned silicon carbide-silicon amyloplastid, is sieved, is uniformly mixed, in 60~100MPa condition
Under suppressed, then under the conditions of 80~90 DEG C drying 12~for 24 hours, obtain aluminium nitride biscuit；
(4) it will be put into sintering furnace after above-mentioned aluminium nitride biscuit, be sintered under the conditions of 1600~2300 DEG C, and 100~
2~5 hours are kept the temperature under the conditions of 1000 DEG C, obtains SiC reinforcement aluminium nitride ceramics.
3. the preparation method of SiC reinforcement aluminium nitride ceramics according to claim 2, which is characterized in that in step (3),
The preparation method of the aluminium nitride amyloplastid includes: that 1) carbon black is dispersed in a certain amount of water, then by aluminum nitrate and
Additive dissolution is scattered in proportion in carbon black solution, after mixing, is heated at a temperature of 100~600 DEG C, and solution occurs anti-
Should after obtain predecessor；2) by the predecessor in 1200~1600 DEG C of flowing nitrogen or ammonia atmosphere carbon thermal reduction 60~
600min obtains carbothermic reduction reaction product；3) the carbothermic reduction reaction product is passed through to the at a temperature of oxygen at 500~800 DEG C
30~600min of carbon is eliminated, aluminium nitride amyloplastid is obtained.
4. the preparation method of SiC reinforcement aluminium nitride ceramics according to claim 2, which is characterized in that the binder
Selected from one of polyvinyl alcohol, polyvinyl butyral, methylcellulose.
5. the preparation method of SiC reinforcement aluminium nitride ceramics according to claim 2, which is characterized in that the binder
Weight be the 0.1~0.2% of silicon carbide and silicon gross weight.
6. the preparation method of SiC reinforcement aluminium nitride ceramics according to claim 3, which is characterized in that in step 1),
The additive is urea, ammonium nitrate, nitric acid.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109928764A (en) * | 2019-02-27 | 2019-06-25 | 郑海东 | A kind of LED light ceramic material and preparation method thereof |
| CN113213942A (en) * | 2021-05-26 | 2021-08-06 | 湖南仁龙特种陶瓷有限公司 | Composite silicon carbide ceramic kiln furniture and preparation method thereof |
| CN114315371A (en) * | 2021-10-25 | 2022-04-12 | 郴州功田电子陶瓷技术有限公司 | Aluminum nitride ceramic substrate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109928764A (en) * | 2019-02-27 | 2019-06-25 | 郑海东 | A kind of LED light ceramic material and preparation method thereof |
| CN113213942A (en) * | 2021-05-26 | 2021-08-06 | 湖南仁龙特种陶瓷有限公司 | Composite silicon carbide ceramic kiln furniture and preparation method thereof |
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| CN114315371A (en) * | 2021-10-25 | 2022-04-12 | 郴州功田电子陶瓷技术有限公司 | Aluminum nitride ceramic substrate |
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